3-氯-1,2-丙二醇及缩水甘油的合成研究

以甘油为原料,在无水乙酸的作用下与HCl反应合成出3-氯-1,2-丙二醇,优化了3-氯-1,2-丙二醇的合成工艺,得到适宜的反应条件为:反应温度90℃,反应时间4 h,催化剂用量5%(w/w),HCl气体流速20 L/h。然后利用制备的3-氯-1,2-丙二醇在二氯甲烷溶剂中与强碱性阴离子交换树脂作用合成了缩水甘油,最佳反应时间为1 h。产物分别通过GC和IR进行了鉴定,3-氯-1,2-丙二醇和缩水甘油的产率分别可达到84.6%和89.6%。

Synthesis of 3-chyloro-1,2-propanediol and glycidyl

3-Chyloro-1,2-propanediol was prepared by glycerine and HCl under the catalysis of acetic anhydride by using glycerinas raw material.The synthesis conditions were optimized and the appropriate reaction conditions were as follows:reaction temperature 90 ℃,reaction time 4 h,amount of catalyst 5%(w/w),HCl gas flow capacity 20 L/h.Then,glycidyl was prepared by 3-chyloro-1,2-propanediol and strong basic ion-exchange in the dichloromethane phase,the best reaction time was 1 h.Both of the products were analyzed with GC and IR,the yelid of 3-chyloro-1,2-propanediol was 84.6% and glyceriol was 89.6% respectively.